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Catalytic or photocatalytic preparation method of parylene af4

a technology of parylene af4 and photocatalysis, which is applied in the preparation of halogenated hydrocarbons, group 5/15 element organic compounds, organic chemistry, etc., can solve the problems of increasing the preparation cost and not being suitable for mass production, and achieve the effect of significantly increasing the production capacity of parylene af4

Active Publication Date: 2014-01-09
YUAN SHIN MATERIALS TECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The present invention provides a method for making parylene AF4 using a catalyst or photocatalytic reaction. This method reduces the reaction time and increases the yield of parylene AF4 by using a high concentrated reaction mixture. The method involves adding a reactant, such as CFB, BFB, or IFB, into a small amount of solvent with a reducing agent, and then adding a catalyst or photocatalyst. The reaction is accelerated by heating and the production of parylene AF4 is significantly increased. This method allows for large-scale production of parylene AF4 with great commercial advantages.

Problems solved by technology

In the previous methods, however, in order to prevent the undesired byproducts formation, the reactions were usually carried out in highly diluted conditions, that is, large amount of solvents are necessary in the synthetic methods, therefore, the purchase and storage of the solvent, the process of feeding and the removal of the solvent or impurities will increase the cost of the preparation, coupled with long reaction time, more byproducts and complication of parylene AF4 purification procedure, those methods are not suitable for mass productions.

Method used

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  • Catalytic or photocatalytic preparation method of parylene af4
  • Catalytic or photocatalytic preparation method of parylene af4
  • Catalytic or photocatalytic preparation method of parylene af4

Examples

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embodiment 1

[0021]This embodiment involves providing a 250 ml three-necked bottle and purging with nitrogen, then adding 75 ml of DMAC solvent, 15.68 g (0.24 mol) of reducing agent zinc powder, and 0.21 g (3.5 mmol) of catalyst KF, stirred and preheated to 120° C. Then 29.64 g (0.12 mol) of reactant CH3 is added dropwise to the reaction bottle, and the reaction temperature is gradually increased to 135° C., the feeding time is about 2 hours and the reaction is continued for 3 hours. The crude product is filtered and washed by DMAC. The double bond-containing byproduct in filtrate is oxidized by potassium permanganate, and the filtrate is concentrated and water is added to the resulting crude solid in order to remove the inorganic substances. The crude solid obtained from filtration and recrystallized in chloroform (CHCl3) to obtain 8.43 g of pure parylene AF4 (purity 99.5%, yield 40.28%). The parylene AF4 product is confirmed by analysis: the molecular weight of 352.0 g / mol is confirmed by GC / M...

embodiment 2

[0022]In this embodiment of the present invention, a 250 ml three-necked bottle is provided and purged with nitrogen, then 50 ml of DMAC solvent is added, 7.84 g (0.12 mol) of reducing agent zinc powder, and 0.10 g (0.6 mmol) of catalyst stirred and preheated to 120° C. Then the mixture of 14.82 g (0.06 mol) of reactant CFB and 1.95 g (0.006 mol) of reactant BFB is added dropwise to the reaction bottle, and the reaction temperature is gradually increased to 140° C., the feeding time is about 1 hour and the reaction is continued for 3 hours. The crude product is purified and analyzed by the same methods of embodiment 1 and 3.58 g of parylene AF4 is obtained (purity 99.63%, yield 31.0%).

embodiment 3

[0023]Provide a 250 ml three-necked bottle and purge with nitrogen, then add 150 ml of DMSO solvent, 7.84 g (0.12 mol) of reducing agent zinc powder, and 0.10 g (0.6 mmol) of catalyst KI, stirred and preheated to 120° C. Then 14.82 g (0.06 mot) of reactant CFB is added dropwise to the reaction bottle, and the reaction temperature is gradually increased to 131° C., the feeding time is about 1 hour and the reaction is continued for 3 hours. The crude product is purified and analyzed by the same methods of embodiment 1 and parylene AF4 is obtained with 99.34% of purity and 26.7% of yield.

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Abstract

The present invention disclosed a preparation method of parylene AF4, which provides a reactant and a reducing agent with the use of catalyst or exposure to UV light with photo-initiator, to shorten the reaction time as a result of minimized the byproduct(s) formation, and obtain high purity (>99.0%) of parylene AF4 product under high concentrated reaction mixture.

Description

BACKGROUND OF THE INVENTION[0001]1. Field of the Invention[0002]The present invention relates to a preparation method of octafluoro-(2,2)-paracyclophane (parylene AF4) and, more particularly, the present invention relates to a catalytic or a photocatalytic preparation method of parylene AF4.[0003]2. Description of Related Art[0004]By using the vacuum pyrolysis chemical vapor deposition (CVD) method, parylene can be made into an extremely thin film which has an excellent uniformity, chemical stability and high transparency. Parylene is widely used in the forms of coating thin film, for application on the electrical isolation of printed circuit board, moisture protection of sensors or medical equipment, insulating layers of electrical unit, various protective films or packing materials, and preventing corrosion of metal coatings.[0005]Recently, due to high melting point (about 450° C.) and low dielectric constant (about 2.2) of the fluorinated parylene polymers, such as poly(tetrafluo...

Claims

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Application Information

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IPC IPC(8): C07C17/269
CPCC07C17/269C07C2603/92C07C23/18
Inventor LIN, CHUN-HSUSUN, CHIEN-YIYIN, YUNG-YULI, CHUN-SHIHCHOU, YO-CHUN
Owner YUAN SHIN MATERIALS TECH CORP